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基于 QuEChERS 的超高效液相色谱-串联质谱法测定血浆中 5 种钙通道阻滞剂

QuEChERS-Based Approach to the Extraction of Five Calcium Channel Blockers from Plasma Determined by UPLC-MS/MS.

机构信息

College of Pharmacy, Hebei Medical University, Shijiazhuang 050000, China.

College of Chemistry and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050000, China.

出版信息

Molecules. 2023 Jan 9;28(2):671. doi: 10.3390/molecules28020671.

DOI:10.3390/molecules28020671
PMID:36677729
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9866929/
Abstract

Here, a QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment method was combined with UPLC-MS/MS to facilitate the rapid and reliable simultaneous detection of five calcium channel blockers (CCBs) in human plasma. For this approach, samples were treated with 1 mL of acetonitrile, 350 mg of magnesium sulfate, and 70 mg of PSA adsorbent prior to centrifugation. Supernatants then underwent gradient elution for 8 min with an Agilent C18 column using an acetonitrile-water solution supplemented with 5 mmol⋅L of ammonium acetate. This technique exhibited a good linear response in the 1-800 ng⋅mL range for the analyzed drugs, with an R≥ 0.9921, an accuracy of 87.54-113.05%, a matrix effect (ME) of 91.21-116.39%, a precision of 0.19-11.64%, and stability of no more than 10.05%. This time-saving QuEChERS reagent-based pretreatment technique thus allowed for the simultaneous and accurate detection of five CCBs in human plasma samples, providing a promising new basis for therapeutic drug monitoring in patients with hypertension.

摘要

这里,一种 QuEChERS(快速、简单、廉价、有效、耐用、安全)预处理方法与 UPLC-MS/MS 相结合,便于快速可靠地同时检测人血浆中的五种钙通道阻滞剂(CCB)。对于这种方法,样品用 1 毫升乙腈、350 毫克硫酸镁和 70 毫克 PSA 吸附剂处理,然后离心。上清液然后用 Agilent C18 柱进行梯度洗脱,使用乙腈-水溶液,补充 5 mmol·L 的乙酸铵,8 分钟即可完成。该技术在分析药物的 1-800 ng·mL 范围内表现出良好的线性响应,R≥0.9921,准确度为 87.54-113.05%,基质效应(ME)为 91.21-116.39%,精密度为 0.19-11.64%,稳定性不超过 10.05%。这种节省时间的基于 QuEChERS 试剂的预处理技术因此允许同时准确地检测人血浆样品中的五种 CCB,为高血压患者的治疗药物监测提供了有前途的新基础。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/aeba48fd8bf0/molecules-28-00671-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/465e9c0fdf42/molecules-28-00671-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/6d762899c6b2/molecules-28-00671-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/9d4b7eac3bb1/molecules-28-00671-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/7d192894a5d9/molecules-28-00671-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/aeba48fd8bf0/molecules-28-00671-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/465e9c0fdf42/molecules-28-00671-g001a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/6d762899c6b2/molecules-28-00671-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/9d4b7eac3bb1/molecules-28-00671-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/7d192894a5d9/molecules-28-00671-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ef24/9866929/aeba48fd8bf0/molecules-28-00671-g006.jpg

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